Trifluoroacetic anhydride → HCID 58137374、化合物

HRID 1907820ノート

反応式

HRID 1907820 の反応式
[CH2:1]([O:3][C:4]1[N:5]=[N+:6]([O-])[C:7]([CH3:13])=[CH:8][C:9]=1[O:10][CH2:11][CH3:12])[CH3:2].FC(F)(F)C(OC(=O)C(F)(F)F)=[O:18]>ClCCl>[CH2:11]([O:10][C:9]1[CH:8]=[C:7]([CH2:13][OH:18])[N:6]=[N:5][C:4]=1[O:3][CH2:1][CH3:2])[CH3:12]

参加物

4

反応物 2

HCID 9845Trifluoroacetic anhydrideHCID 58137375HCID 58137375、化合物

生成物 1

HCID 58137374HCID 58137374、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3,4-Diethoxy-6-methylpyridazine 1-oxide (1.44 g) was initially charged in dichloromethane (50 ml) and admixed dropwise at RT with trifluoroacetic anhydride (2.5 ml). After 2.5 h, the mixture was concentrated to dryness and the residue was taken up with ethanol and saturated potassium carbonate solution. After stirring at RT for 4 h, the mixture was concentrated to dryness again and the residue was admixed with water and dichloromethane. Removal of the organic phase was followed by extraction twice more with dichloromethane, and the combined organic phases were dried over magnesium sulfate, filtered and concentrated. The residue was purified twice using silica gel with dichloromethane/methanol as the eluent. The product-containing fractions were combined and dried. 716 mg of the desired product were obtained.

後処理

  1. concentrationthe mixture was concentrated to dryness
  2. concentrationthe mixture was concentrated to dryness again
  3. customRemoval of the organic phase
  4. extractionwas followed by extraction twice more with dichloromethane
  5. dry with materialthe combined organic phases were dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was purified twice using silica gel with dichloromethane/methanol as the eluent
  9. customdried

出典と根拠

ORDレコード
ord-3dcfb6ad95974df29e5c5834076b3228
出典データセット
uspto-grants-2013_12
特許番号
US08598177B2

反応ノート

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